反应详情

温度

180 °C

Trifluoromethane sulfonic acid 1-ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-7-yl ester(0.40 g), ethyl acrylate(0.13 g), dichlorobis(triphenylphosphine) Palladium (II) (35 mg),lithium chloride(64 mg), and triethylamine(0.19 ml) were added to DMF(4 ml). The mixture was heated at 180° C. (microwave reactor) for 20 minutes. The reaction liquid was cooled to room temperature, and subjected to celite filtration. The filtrate was condensed under reduced pressure, and the residue was purified by silica gel column chromatography (hexane: ethyl acetate=70:30→30:70). The purified product was condensed under reduced pressure to give the title compound(0.36 g) as a pale yellow solid.

1. customThe reaction liquid
2. temperaturewas cooled to room temperature
3. filtrationsubjected to celite filtration
4. customcondensed under reduced pressure
5. customthe residue was purified by silica gel column chromatography (hexane: ethyl acetate=70:30→30:70)
6. customcondensed under reduced pressure